CN105590757A - Carbon nanotube/graphene composite gel and preparation method thereof - Google Patents
Carbon nanotube/graphene composite gel and preparation method thereof Download PDFInfo
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- CN105590757A CN105590757A CN201410657384.4A CN201410657384A CN105590757A CN 105590757 A CN105590757 A CN 105590757A CN 201410657384 A CN201410657384 A CN 201410657384A CN 105590757 A CN105590757 A CN 105590757A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a carbon nanotube/graphene composite gel. In the carbon nanotube/graphene composite gel, carbon nanotubes are inserted into the graphene gel to form three-dimensional porous structure, thereby contributing to prevention of graphene interlayer agglomeration, increasing surface area, and improving the electrochemical performance of the carbon nanotube/graphene composite gel. A method for preparing the carbon nanotube/graphene composite gel comprises adding carbon nanotubes to a graphene oxide aqueous solution and dispersing the carbon nanotubes uniformly by a hydrothermal method; obtaining the carbon nanotube/graphene oxide composite gel by using thermal treatment; and obtaining the carbon nanotube/graphene composite gel by using reducing, cleaning, and drying methods. An experiment testifies that the carbon nanotube/graphene composite gel has higher conductivity than graphene gel and can be used as an electrode material. Used as the electrode material of a super capacitor, the carbon nanotube/graphene composite gel increases the specific capacitance and the power density of the super capacitor.
Description
Technical field
The present invention relates to Graphene gel technique field, relate in particular to a kind of CNT/Graphene plural gel and preparation thereofMethod.
Background technology
Graphene be carbon atom on two dimensional surface with sp2The carbon material of the monatomic bed thickness that hydridization form is interconnected to formMaterial, its carbon atom is hexagon cellular shape and arranges. Due to its special structural behaviour, Graphene has much good physicsAnd chemical property, such as high mechanical strength (～1TPa) [referring to (a) C.Lee, X.D.Wei, J.W.Kysar, J.Hone,Science, 321 (2008) 385-388.], good electric conductivity and thermal conductivity [referring to: (b) P.Avouris, Z.H.Chen, V.Perebeinos,NatNanotechnol,2(2007)605-615.(c)K.S.Novoselov,A.K.Geim,S.V.Morozov,D.Jiang,Y.Zhang,S.V.Dubonos,I.V.Grigorieva,A.A.Firsov,Science,306(2004)666-669.] and large specific area (2675m2g-1). These good performances make Graphene be suitable as super capacitorElectrode material in device. But Graphene is easily reunited in preparation process, causes specific area lower than theoretical value, simultaneouslyBe unfavorable for that ion enters between graphene layer, thereby affected its chemical property.
Graphene gel is owing to having high specific area, suitable microcellular structure and multiple electric transmission path, and extensivelyBe used as the electrode material of ultracapacitor. Utilize hydro-thermal method [referring to (d) Y.Zhao, C.G.Hu, Y.Hu, H.H.Cheng,G.Q.Shi, L.T.Qu, AngewChemIntEdit, 51 (2012) 11371-11375.], template [referring to: (e) S.H.Lee,H.W.Kim,J.O.Hwang,W.J.Lee,J.Kwon,C.W.Bielawski,R.S.Ruoff,S.O.Kim,AngewChemIntEdit, 49 (2010) 10084 ?10088.] and chemical reduction method [referring to (f) X.T.Zhang, Z.Y.Sui, B.Xu, S.F.Yue,Y.J.Luo, W.C.Zhan, B.Liu, JMaterChem, 21 (2011) 6494-6497.] etc. all can synthesizing graphite alkene gel.But the solidifying electric conductivity of Graphene is generally at 1-100Sm-1Magnitude, still needs during as the electrode material of ultracapacitorFurther improve.
Summary of the invention
The present invention is directed to the lower problem of above-mentioned Graphene gel electric conductivity, aim to provide a kind of stone with satisfactory electrical conductivityChina ink alkene gel.
For this reason, the inventor is attached to carbon nano-tube material in Graphene gel, forms the carbon nanometer with special constructionPipe/Graphene plural gel, utilizes the electric conductivity that CNT is good, and its electrical conductivity is generally 104Sm-1Magnitude, andImprove the electric conductivity of plural gel.
That is, the technical solution adopted in the present invention is: a kind of CNT/Graphene plural gel, wherein CNT is wornBe inserted in Graphene gel, form three-dimensional porous structure.
Described CNT includes but not limited to SWCN and/or multi-walled carbon nano-tubes, is preferably single wall carbon nano-tubePipe.
The present invention also provides a kind of method of preparing above-mentioned CNT/Graphene plural gel, adopts hydro-thermal method, at oxygenIn the functionalized graphene aqueous solution, add CNT, specifically comprise the steps:
(1) graphene oxide is dispersed in water, obtains graphite oxide aqueous solution;
(2) CNT is added in graphite oxide aqueous solution, be uniformly dispersed, obtain CNT/graphene oxideDispersion liquid; Or, first even carbon nanotube is scattered in water, obtain carbon nano tube dispersion liquid, soAfter by carbon nano tube dispersion liquid and graphene oxide aqueous solution, make even carbon nanotube be dispersed in mixingIn solution, obtain CNT/graphene oxide dispersion liquid;
(3) utilize hydro-thermal method, CNT/graphite oxide dispersion liquid is heat-treated, obtain CNT/oxidationGraphene plural gel;
(4) utilize reducing agent reduction CNT/graphene oxide plural gel, then wash, be dried, obtain carbon and receiveMitron/Graphene plural gel.
As preferably, in described step (1), the source of graphene oxide is not limit, and can select commercially available oxidation stoneChina ink alkene, also can adopt graphite is that raw material is prepared graphene oxide by oxidation reaction, Hummers-Offeman legal system is standbyGraphene oxide is method conventional in this area.
In described step (2), in CNT/graphene oxide dispersion liquid, the matter of graphene oxide and CNTAmount ratio is preferably at 3～30 o'clock, and synthetic CNT/Graphene gel has good electric conductivity and suitable many simultaneouslyPore structure.
As preferably, in described step (3), heat treatment temperature is 90 DEG C～200 DEG C, heat treatment time be 8h～20h。
As preferably, in described step (4), reducing agent is not limit, and comprises hydrazine hydrate aqueous solution, hydrogen iodide, hydrogenationThe mixing of one or more in aluminium lithium, sodium borohydride, ascorbic acid, highly basic, azanol, Dimethylhydrazine etc.
In sum, the present invention carries out CNT and Graphene gel compound, utilizes the architectural feature of CNT,Form three-dimensional porous structure, be conducive to avoid reuniting between graphene layer, improve its surface area low, thereby improve its electrochemistryPerformance. Experiment confirmation, with Graphene gel phase ratio, this CNT/Graphene plural gel has higher electric conductivity,Can be used as electrode material and use, in the time using as electrode material for super capacitor, improved the ratio electricity of ultracapacitorHold and power density.
Brief description of the drawings
Fig. 1 is the CNT/graphene oxide dispersion liquid in embodiment 1, and the carbon forming after hydro-thermal reaction is receivedThe picture of mitron/Graphene gel;
Fig. 2 is native graphite, graphene oxide, and the Graphene gel that comparative example 1 makes and embodiment 1 makeThe electron diffraction diagram of CNT/Graphene plural gel;
Fig. 3 is the scanning electron microscope (SEM) photograph of CNT/Graphene plural gel of making of embodiment 1;
Fig. 4 is the transmission electron microscope picture of CNT/Graphene plural gel of making of embodiment 1;
Fig. 5 (a) is CNT/Graphene gel of making of embodiment 1 following during as electrode material for super capacitorRing volt-ampere curve;
Fig. 5 (b) is CNT/Graphene plural gel and the comparative example 1 who makes in embodiment 1 and embodiment 2In the Graphene gel that the makes charging and discharging curve during as electrode material for super capacitor;
Fig. 5 (c) is the graphite that CNT/Graphene plural gel of making of embodiment 1 and comparative example 1 makeRatio electric capacity-the current density of alkene gel during as electrode material for super capacitor relatively schemed;
Fig. 5 (d) is the graphite that CNT/Graphene plural gel of making of embodiment 1 and comparative example 1 makeThe AC impedance spectrogram of alkene gel during as electrode material for super capacitor.
Detailed description of the invention
Embodiment 1:
The present embodiment provides a kind of CNT/Graphene plural gel, and it has three-dimensional porous structure, and wherein single wall carbon is receivedMitron interts in Graphene gel.
The preparation method of this CNT/Graphene plural gel is as follows:
(1) getting 10000 object native graphites is raw material, adopts Hummers-Offeman legal system for graphite oxide; ThenThe graphite oxide obtaining is mixed with to the aqueous solution of 4mg/ml, then adopts the ultrasonic processing of supersonic cleaning machine 3h, be oxidizedGraphene aqueous solution;
(2) get the above-mentioned graphene oxide solution of 15ml in sample bottle, then add the single armed CNT of 3mg, superSound 2h obtains CNT/graphene oxide uniform dispersion, as shown in the Image to left in Fig. 1;
(3) sample bottle is transferred in reactor, reactor is placed on to 180 DEG C of reaction 12h in constant temperature oven, then certainlySo be cooled to room temperature, obtain CNT/Graphene plural gel, taken out washing after put into the sample that fills the aqueous solutionIn bottle, obtain CNT/Graphene plural gel aqueous solution, as shown in the Image to right in Fig. 1, can find out hydro-thermalAfter reaction, form regular CNT/Graphene gel;
(4) to the hydrazine hydrate aqueous solution that adds 1mL85% in CNT/Graphene plural gel aqueous solution, be placed onIn constant temperature oven, 95 DEG C of reaction 12h, then naturally cooling, deionized water cyclic washing CNT/Graphene plural gel,Finally carry out freeze drying, obtain dry carbon mitron/Graphene plural gel.
Embodiment 2:
The present embodiment provides a kind of CNT/Graphene plural gel, and it has three-dimensional porous structure, and wherein single wall carbon is receivedMitron interts in Graphene gel.
The preparation method of this CNT/Graphene plural gel is as follows:
(1) identical with the step of (1) in embodiment 1;
(2) get the above-mentioned graphene oxide solution of 15ml in sample bottle, then add the single armed CNT of 30mg, superSound 2h obtains CNT/graphene oxide uniform dispersion;
(3) sample bottle is transferred in reactor, reactor is placed on to 180 DEG C of reaction 12h in constant temperature oven, then certainlySo be cooled to room temperature, obtain CNT/Graphene plural gel, taken out washing after put into the sample that fills the aqueous solutionIn bottle, obtain CNT/Graphene plural gel aqueous solution;
(4) identical with the step of (4) in embodiment 1.
Comparative example 1:
The present embodiment is the comparative example of embodiment 1.
The present embodiment provides a kind of Graphene gel, and its preparation method is as follows:
(1) identical with the step (1) in embodiment 1;
(2) get the above-mentioned graphene oxide solution of 15ml in sample bottle;
(3) sample bottle is transferred in reactor, reactor is placed on to 180 DEG C of reaction 12h in constant temperature oven, thenNaturally cool to room temperature, obtain Graphene gel, taken out washing after put into the sample bottle that fills the aqueous solution, obtainGraphene gel solution;
(4), to the hydrazine hydrate aqueous solution that adds 1mL85% in Graphene gel solution, be placed in constant temperature oven 95 DEG CReaction 12h, then naturally cooling, deionized water cyclic washing Graphene gel, finally carries out freeze drying, is doneDry Graphene gel.
To the graphite making in the CNT/Graphene plural gel making in above-described embodiment 1 and 2 and comparative example 1Alkene gel is tested.
Fig. 2 is native graphite, graphene oxide, and the Graphene gel making in comparative example 1, and in embodiment 1The electron diffraction diagram of the CNT/Graphene gel making. Can find out, in embodiment 1, CNT/Graphene is compoundIn the diffraction maximum of gel and comparative example 1, the diffraction maximum of Graphene gel and the diffraction maximum of graphene oxide are obviously notWith; The diffraction of Graphene gel in the diffraction maximum of CNT/Graphene plural gel and comparative example 1 in embodiment 1Peak approaches the diffraction maximum of native graphite, illustrates that graphene oxide is reduced to Graphene.
Fig. 3 and Fig. 4 are respectively scanning electron microscope (SEM) photograph and the transmission electron microscope pictures of CNT/Graphene plural gel in embodiment 1.Can find out, CNT/Graphene plural gel has three-dimensional porous structure, and wherein even carbon nanotube is interted at graphiteIn alkene gel structure, form three-dimensional CNT/Graphene plural gel.
Fig. 5 (a) is that CNT/Graphene plural gel of making in embodiment 1 is as electrode material for super capacitorTime cyclic voltammetry curve. Can find out, under different scanning rates, curve all forms good rectangle, and this electricity is describedUtmost point material has typical electric double layer capacitance, has good chemical property.
Fig. 5 (b) is CNT/Graphene plural gel and the comparative example 1 who makes in embodiment 1 and embodiment 2In the Graphene gel that the makes charging and discharging curve during as electrode material for super capacitor. Can find out curve 1,2With 3 all there is good linearity and symmetry, illustrate that these three kinds of electrode materials have good chemical property; With contrastGraphene gel phase ratio in embodiment 1, the discharge process slope of the CNT/Graphene gel in embodiment 1 definitelyBe worth littlely, illustrate that in embodiment 1, CNT/Graphene plural gel has higher ratio electric capacity. With comparative example 1Middle Graphene gel phase ratio, the absolute value of the discharge process slope of the CNT/Graphene gel in embodiment 2 is larger,Illustrate that the ratio electric capacity of CNT/Graphene plural gel in embodiment 2 is on the contrary than the Graphene gel in comparative example 1Ratio electric capacity little. This illustrates in the time of the too high levels of CNT, can reduce on the contrary the ratio electric capacity of Graphene gel. Through realityChecking, in CNT/graphene oxide dispersion liquid, controls the quality ratio of graphene oxide and CNT 3～30Scope is advisable.
Fig. 5 (c) makes in CNT/Graphene plural gel of making in embodiment 1 and comparative example 1Ratio electric capacity-the current density of Graphene gel during as electrode material for super capacitor relatively schemed. Can find out, with graphiteAlkene gel phase ratio, CNT/Graphene plural gel electrode higher than electric capacity conservation rate. CNT/Graphene is describedGel electrode has better high rate performance.
Fig. 5 (d) makes in CNT/Graphene plural gel of making in embodiment 1 and comparative example 1The AC impedance spectrogram of Graphene gel during as electrode material for super capacitor. Can find out, with Graphene gel phase ratio,CNT/Graphene gel during as electrode material for super capacitor the intercept of impedance spectrum and real axis less, equivalent string is describedConnection resistance is less, and power density is significantly improved.
To sum up analyze, the CNT/Graphene plural gel making in embodiment 1 has three-dimensional porous structure, with graphiteThe electric conductivity that alkene gel phase is higher than having, in the time using as electrode material for super capacitor, has improved ultracapacitorRatio electric capacity and power density; The content of CNT has impact to the performance of material simultaneously, should be controlled at certain limitIn.
Above-described embodiment has been described in detail technical scheme of the present invention, is understood that and the foregoing is onlySpecific embodiments of the invention, are not limited to the present invention, all any amendments of making within the scope of principle of the present invention,Supplementary or similar fashion is alternative etc., within all should being included in protection scope of the present invention.
Claims (8)
1. CNT/Graphene plural gel, is characterized in that: CNT interts in Graphene gel, structureBecome three-dimensional porous structure.
2. CNT/Graphene plural gel as claimed in claim 1, is characterized in that: described CNT is for singleWall carbon nano tube and/or multi-walled carbon nano-tubes.
3. the method for preparation CNT/Graphene plural gel as claimed in claim 1 or 2, is characterized in that: bagDraw together following steps:
(1) graphene oxide is dispersed in water, obtains graphite oxide aqueous solution;
(2) CNT is added in graphite oxide aqueous solution, be uniformly dispersed, obtain CNT/graphene oxideDispersion liquid; Or, first even carbon nanotube is scattered in water, obtain carbon nano tube dispersion liquid, soAfter by carbon nano tube dispersion liquid and graphene oxide aqueous solution, make even carbon nanotube be dispersed in mixingIn solution, obtain CNT/graphene oxide dispersion liquid;
(3) utilize hydro-thermal method, CNT/graphite oxide dispersion liquid is heat-treated, obtain CNT/oxidationGraphene plural gel;
(4) utilize reducing agent reduction CNT/graphene oxide plural gel, then wash, be dried, obtain carbon and receiveMitron/Graphene plural gel.
4. the preparation method of CNT/Graphene plural gel as claimed in claim 3, is characterized in that: described stepSuddenly in (2), in CNT/graphene oxide dispersion liquid, the quality ratio of graphene oxide and CNT is 3～30.
5. the preparation method of CNT/Graphene plural gel as claimed in claim 3, is characterized in that: described step(3) in, heat treatment temperature is 90 DEG C～200 DEG C, and heat treatment time is 8h～20h.
6. the preparation method of CNT/Graphene plural gel as claimed in claim 3, is characterized in that: described step(4) in, reducing agent be hydrazine hydrate aqueous solution, hydrogen iodide, lithium aluminium hydride reduction, sodium borohydride, ascorbic acid, highly basic,The mixing of one or more in azanol, Dimethylhydrazine.
7. CNT/Graphene plural gel as claimed in claim 1 or 2 is as the application of electrode material.
8. CNT/Graphene plural gel as claimed in claim 7, as the application of electrode material, is characterized in that:Described electrode material is electrode material for super capacitor.
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| CN106252634A (en) * | 2016-09-24 | 2016-12-21 | 上海大学 | Graphene aerogel load CNT and ZIF 67 electrode material of lithium battery preparation method |
| CN106783197A (en) * | 2016-11-16 | 2017-05-31 | 东华大学 | Pyrolysis porous carbon graphene composite materials of a kind of ZIF 8 and its preparation method and application |
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| CN106783197A (en) * | 2016-11-16 | 2017-05-31 | 东华大学 | Pyrolysis porous carbon graphene composite materials of a kind of ZIF 8 and its preparation method and application |
| CN108117437A (en) * | 2016-11-29 | 2018-06-05 | 沙特基础工业全球技术公司 | Fertilizer composition of controlled release and application thereof |
| CN108251076A (en) * | 2016-12-29 | 2018-07-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nanotube-graphene composite radiating film, preparation method and application |
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| CN107381546A (en) * | 2017-07-25 | 2017-11-24 | 常州大学 | The method that one step hydro thermal method prepares carbon nano tube/graphene hydridization conductive material |
| CN107565140A (en) * | 2017-10-31 | 2018-01-09 | 武汉理工大学 | Preparation method for the three-dimensional porous graphene carbon nanotube electrode of enzymatic |
| CN109841428A (en) * | 2017-11-27 | 2019-06-04 | 中国电子科技集团公司第十八研究所 | Preparation method of high-density graphene electrode material for lithium ion capacitor |
| CN108439389A (en) * | 2018-04-11 | 2018-08-24 | 同济大学 | A kind of preparation method of the carbon nano tube/graphene foam with Meta Materials performance |
| CN108786729A (en) * | 2018-06-06 | 2018-11-13 | 张小伏 | The preparation method of mask graphene/active carbon in-situ plural gel adsorbent |
| CN109721048A (en) * | 2019-01-22 | 2019-05-07 | 国网冀北电力有限公司秦皇岛供电公司 | A kind of preparation method of three-dimensional globular conductive graphene/carbon nano tube compound material |
| CN110797202A (en) * | 2019-09-26 | 2020-02-14 | 威海三合永新能源科技有限公司 | Carbon nanotube/graphene/activated carbon composite electrode material and preparation method and application thereof |
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